US5853801A - Process for the preparation of continuous optical compensatory sheet - Google Patents
Process for the preparation of continuous optical compensatory sheet Download PDFInfo
- Publication number
- US5853801A US5853801A US08/697,888 US69788896A US5853801A US 5853801 A US5853801 A US 5853801A US 69788896 A US69788896 A US 69788896A US 5853801 A US5853801 A US 5853801A
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- Expired - Lifetime
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/12—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by mechanical means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/02—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber
- B05D7/04—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber to surfaces of films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/07—Flat, e.g. panels
- B29C48/08—Flat, e.g. panels flexible, e.g. films
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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- B32B38/162—Cleaning
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K19/00—Liquid crystal materials
- C09K19/02—Liquid crystal materials characterised by optical, electrical or physical properties of the components, in general
- C09K19/0208—Twisted Nematic (T.N.); Super Twisted Nematic (S.T.N.); Optical Mode Interference (O.M.I.)
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- G02B5/30—Polarising elements
- G02B5/3016—Polarising elements involving passive liquid crystal elements
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1337—Surface-induced orientation of the liquid crystal molecules, e.g. by alignment layers
- G02F1/13378—Surface-induced orientation of the liquid crystal molecules, e.g. by alignment layers by treatment of the surface, e.g. embossing, rubbing or light irradiation
- G02F1/133784—Surface-induced orientation of the liquid crystal molecules, e.g. by alignment layers by treatment of the surface, e.g. embossing, rubbing or light irradiation by rubbing
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/137—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells characterised by the electro-optical or magneto-optical effect, e.g. field-induced phase transition, orientation effect, guest-host interaction or dynamic scattering
- G02F1/139—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells characterised by the electro-optical or magneto-optical effect, e.g. field-induced phase transition, orientation effect, guest-host interaction or dynamic scattering based on orientation effects in which the liquid crystal remains transparent
- G02F1/1396—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells characterised by the electro-optical or magneto-optical effect, e.g. field-induced phase transition, orientation effect, guest-host interaction or dynamic scattering based on orientation effects in which the liquid crystal remains transparent the liquid crystal being selectively controlled between a twisted state and a non-twisted state, e.g. TN-LC cell
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
- B29K2105/0079—Liquid crystals
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
- G02F1/13363—Birefringent elements, e.g. for optical compensation
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F2413/00—Indexing scheme related to G02F1/13363, i.e. to birefringent elements, e.g. for optical compensation, characterised by the number, position, orientation or value of the compensation plates
- G02F2413/10—Indexing scheme related to G02F1/13363, i.e. to birefringent elements, e.g. for optical compensation, characterised by the number, position, orientation or value of the compensation plates with refractive index ellipsoid inclined, or tilted, relative to the LC-layer surface O plate
Definitions
- the present invention relates to a process for the preparation of a continuous optical compensatory sheet which is useful for improving image contrast and viewing angle of a liquid crystal display.
- LCDs liquid crystal displays
- An LCD generally has a structure of a liquid crystal cell disposed between a pair polarizing sheets. Most of LCDs use a twisted nematic liquid crystal. The operational mode of LCDs using a twisted nematic liquid crystal is divided into a birefringence mode and an optical rotatory mode.
- a super twisted nematic liquid crystal display (hereinafter referred to as STN-LCD) utilizing the birefringence mode uses a super twisted nematic liquid crystal which shows a twisted angle of more than 90 degrees and having steep electro-optical characteristics.
- STN-LCD therefore, has an advantage of displaying a large area by driving in time-sharing mode.
- practical contrast of image is obtained in a yellow mode (yellowish green/dark blue) or a blue mode (blue/light yellow), and therefore to obtain a white/black mode, an optical compensatory sheet (mono-axial stretched polymer film or liquid crystal cell for compensation) is required to attach to the STN-LCD.
- a twisted nematic liquid crystal showing a twisted angle of 90 degrees and having positive birefringence is employed for displaying an image.
- This is called LCD of an optically rotary mode (i.e., TN-LCD).
- TN-LCD display mode shows quick response (such as several tens of milliseconds) and high display contrast, and easily provides a black-white display of high contrast.
- the optical rotatory mode has a number of advantages compared with the birefringence mode or other modes.
- TN-LCD display generally has no optical compensatory sheet.
- TN-LCD has disadvantages that coloring or contrast on display varies depending upon viewing angle to a liquid crystal display, and its display characteristics are not comparable to the display characteristics of CRT.
- phase difference film optical compensatory sheet
- optical compensatory sheets proposed in these Publications give no optical effect when a liquid crystal display is seen from the direction vertical to a screen of the display because phase difference in the direction perpendicular to a surface of the liquid crystal display is almost zero.
- the optical compensatory sheet serves for compensation of phase difference (depending upon wavelengths of light) that occurs when the liquid crystal display is viewed from oblique directions.
- the phase difference results in unfavorable viewing angle characteristics such as coloring and disappearance of displayed image in the oblique directions.
- optical compensatory sheet is needed to have negative birefringence for compensating positive birefringence of the twisted nematic liquid crystal and an inclined optic axis.
- Japanese Patent Provisional Publications No. 4(1992)169539 and No. 4(1992)-276076, and EP0576304 A1 disclose an optical compensatory sheet having the negative birefringence and inclined optic axis.
- the disclosed sheet is prepared by stretching a polymer such as polycarbonate or polyester and has the directions of the main refractive indices which are inclined from the normal of the sheet.
- To prepare the above sheet by the stretching treatment extremely complicated treatments are required. Therefore an optical compensatory sheet of a large surface area cannot be easily prepared according to the disclosed process.
- an optical compensatory sheet comprising a liquid crystalline polymer.
- Japanese Patent Provisional Publications No. 3(1991)-9326 and No. 3(1991)-291601 disclose an optical compensatory sheet for LCD which is prepared by coating a solution of a polymer showing liquid crystal property on an orientation layer provided on a support film.
- the polymer showing liquid crystal property is not satisfactorily oriented on the orientation layer.
- the polymer does not generally show negative birefringence.
- the resulting compensatory sheet scarcely enlarges the viewing angle from all directions.
- Japanese Patent Provisional Publication No. 5(1993)-215921 discloses the use of a birefringence plate (optical compensatory sheet) comprising a support and a polymerizable lod-like compound which shows the liquid crystal property and positive birefringence.
- the birefringence plate is prepared by coating a solution of the lod-like compound on the support and curing the compound under heating.
- the cured layer dose not show the sheet scarcely enlarges the viewing angle from all directions.
- the above known optical compensatory sheets comprising a support film, an orientation layer of the polymer and a liquid crystalline compound layer cannot greatly enlarge the viewing angle from all directions.
- EP 646829 A1 discloses a liquid crystal display provided with an optical compensatory sheet greatly enlarging the viewing angle from all directions.
- the optical compensatory sheet has a representative structure comprising a transparent support, an orientation layer such as a rubbed polyvinyl alcohol layer thereon, and an optically anisotropic layer of a discotic liquid crystalline compound provided on the orientation layer. The use of the discotic liquid crystalline compound is stated to bring about enlargement of the viewing angle.
- the optical compensatory sheet is, for example, prepared by a process comprising the steps of forming a transparent resin layer for orientation layer on a transparent support by coating method, subjecting the transparent resin layer to rubbing treatment to form an orientation layer, forming a layer of discotic compound having liquid crystalline property on the orientation layer by coating method, and heating the coated layer to form a discotic nematic phase.
- the steps each are independently performed and therefore the process comprising the steps is not suitable for industrial production of the optical compensatory sheet.
- a coating liquid of a resin for forming an orientation layer in a solvent on a surface of a moving continuous transparent film (i.e., a continuous transparent film which is in motion) to form a coated layer;
- step iv) is conducted by coating a coating liquid of a polymerizable discotic compound having liquid crystalline property in a solvent on the orientation layer to form a coated layer; and the step vi) is conducted by heating the coated layer to form a discotic nematic phase and exposing the layer of discotic nematic phase to light so as to polymerize the discotic compound.
- step iii) is conducted by subjecting the transparent resin layer to the rubbing treatment while removing dust from the rubbing roller to impart orientation property to the transparent resin layer, whereby an orientation layer is formed, and then removing dust from the orientation layer.
- step iii) is conducted by bringing a surface of the transparent resin layer of the continuous transparent film into contact with a rubbing sheet provided on the rubbing roller under rotation while removing dust on the rubbing sheet, to impart orientation property to the transparent resin layer, whereby an orientation layer is formed, and then removing dust from the orientation layer.
- step iv) is conducted by
- the wire-bar coating machine comprising the wire-bar rotatable around its axis, a coating liquid-circulating device and a coating liquid-holding vessel which has a primary liquid well for the coating liquid fed from the circulating machine, a secondary liquid well for the coating liquid to be fed into the circulating machine and a wall dividing the primary liquid well and the secondary liquid well,
- the wire-bar of the wire-bar coating machine being rotated with feeding the coating liquid into the coating liquid holding vessel.
- step v) is conducted by vaporizing the solvent from the coated layer under sealing the coated layer with a gaseous layer.
- step vi) is conducted by heating the coated layer to form a discotic nematic phase, whereby a layer of discotic compound is formed, and checking the transparent film having the layer of discotic compound on an orientation condition of the layer of discotic compound through continuously measuring the optical characteristics of the transparent film.
- the layer of discotic compound has discotic structure units which have planes inclined from a plane of the transparent film at angles varying along a direction of depth of the optically anisotropic layer.
- nx and ny are main refractive indices on the plane of the support
- nz is a main refractive index in a thickness direction of the support
- d is the thickness of the support in terms of nm (preferably has a light transmittance of not less than 80%).
- a transparent resin layer of a moving continuous transparent film having the transparent resin layer thereon i.e., a continuous transparent film having the transparent resin layer thereon under running
- rubbing treatment by the use of a rubbing roller to impart orientation property to the transparent resin layer, whereby an orientation layer is obtained
- step ii) is conducted by coating a coating liquid of a polymerizable discotic compound having liquid crystalline property in a solvent on the orientation layer to form a coated layer; and the step iv) is conducted by heating the coated layer to form a discotic nematic phase and exposing the coated layer of discotic nematic phase to light so as to polymerize the discotic compound.
- step i) is conducted by bringing a surface of the transparent resin layer of the moving continuous transparent film into contact with a rubbing sheet of the rubbing roller under revolution with removing dust on the rubbing sheet, to impart orientation property to the transparent resin layer, whereby an orientation layer is formed, and then removing dust from the orientation layer.
- step ii) is conducted by
- the wire-bar coating machine comprising the wire-bar rotatable around its axis, a coating liquid-circulating device and a coating liquid holding vessel which has a primary liquid well for the coating liquid fed from the circulating device, a secondary liquid well for the coating liquid to be fed into the circulating device and a wall dividing the primary liquid well and the secondary liquid well,
- the wire-bar of the wire-bar coating machine being rotated with feeding the coating liquid into the coating liquid-holding vessel.
- step iii) is conducted by vaporizing the solvent from the coated layer under sealing the coated layer with a gaseous layer.
- the wire-bar coating machine comprising a wire-bar rotatable around its axis, a coating liquid-circulating device and the coating liquid-holding vessel which has a primary liquid well for the coating liquid fed from the circulating machine, a secondary liquid well for the coating liquid to be fed into the circulating machine and a wall dividing the primary liquid well and the secondary liquid well;
- step i) is conducted by revolving the wire-bar of the wire-bar coating machine with feeding a coating liquid of a discotic compound having liquid crystalline property provided with a polymerizable group in a solvent into the coating liquid holding vessel; and the step iv) is conducted by heating the coated layer to form a discotic nematic phase and curing the coated layer of discotic nematic phase, whereby a layer of discotic compound is formed.
- step iii) is conducted by vaporizing the solvent from the coated layer under sealing the coated layer with a gaseous layer.
- the coating liquid contains the discotic compound in an amount of 15 to 50 weight %, and has a viscosity of 1 to 20 mpa.s at 25° C.
- step iv) is conducted by heating the coated layer by applying heated gas or infrared rays to both sides (surfaces) of the transparent film to form a discotic nematic phase, whereby a layer of discotic compound is formed.
- a continuous optical compensatory sheet having a layer of discotic compound can be efficiently prepared. Therefore the process of the invention is suitable as a process for industrial preparation of the optical compensatory sheet or for mass production of the sheet.
- a continuous optical compensatory sheet obtained by the process of the invention has a uniformly oriented discotic compound layer almost free from adhesion of dust and occurrence of variation of a thickness of the sheet. Therefore, the process of the invention enables preparation in high productivity of the continuous optical compensatory sheet which gives a liquid crystal display almost free from nonuniformity of image. Thus, the process enables mass production of the continuous optical compensatory sheet having good optical characteristics.
- FIG. 1 is a view schematically showing an example of the process for the continuous preparation of the continuous optical compensatory sheet of the invention.
- FIG. 2 is a view schematically showing another example of the process for the continuous preparation of the continuous optical compensatory sheet of the invention.
- FIG. 3 is a view schematically showing an example of the process for the formation of the transparent resin layer for forming an orientation layer.
- FIG. 4 is a sectional view of extrusion die employable for the formation of the transparent resin layer for forming an orientation layer.
- FIG. 5 is a view schematically showing an example of rubbing machine of employable for forming an orientation layer.
- FIG. 6 is a view schematically showing an example of dust-removing device employable in the invention.
- FIG. 7 is a view schematically showing another example of dust-removing device employable in the invention.
- FIGS. 8 to 9 are views schematically showing the a wire-bar coating machine for coating a coating liquid for forming a layer of discotic compound.
- FIG. 10 is view schematically showing inside of the viscosity-control chamber of the wire-bar coating machine.
- FIG. 11 is a view schematically showing the process for the preparation of a layer of discotic compound.
- FIG. 12 is a view schematically showing an example of an ultraviolet irradiation device.
- FIG. 13 is a view schematically showing another example of an ultraviolet irradiation device.
- FIG. 14 is a view schematically showing a representative structure of the optical compensatory sheet obtained by the process of the invention.
- FIG. 15 is a view schematically showing a representative structure of the liquid crystal display having the optical compensatory sheet obtained by the process of the invention.
- the process for the preparation of a continuous optical compensatory sheet according to the invention is characterized in that at least the steps of from a step of subjecting a transparent resin layer of a continuous transparent film having the transparent resin layer thereon to rubbing treatment to a step of winding up the transparent film having the orientation layer and the layer of discotic compound, are continuously performed (i.e., performed in nonstop process). Further, it is preferred that the steps of from a step of feeding the transparent film which is conducted before the step of subjecting the transparent resin layer to rubbing treatment to a step of winding up the transparent film, are continuously performed.
- Another process for the preparation of a continuous optical compensatory sheet according to the invention is characterized in that at least the steps of from a step of coating the coating liquid of a discotic compound utilizing the specific wire-bar coating machine to a step of winding up the transparent film, are continuously performed.
- the continuous operation of the process not only enables mass-production but also depresses adhesion of dust and occurrence of wrinkles (bringing about variation of thickness).
- the process can be, for example, performed according to following steps:
- a step of cooling the layer of discotic compound to solidify preferably rapidly cooling the layer of discotic compound to solidify, or curing the discotic compound (in the case of using as the compound a discotic compound having a polymerizable group) by the means of light or heat energy and cooling the layer of discotic compound (cured layer);
- FIG. 1 schematically shows an example of the process for the preparation of the continuous optical compensatory sheet of the invention.
- the continuous transparent film 4a is fed from a roll of continuous film 5a using a delivery machine 1a, and driven using a driving roller. After dust on a surface of the film is removed using a surface dust-removing machine 2, a coating liquid of a resin for forming an orientation layer in a solvent is coated using a coater 3 on the surface of the film, and the coated layer is dried in a drying zone 5 to form a transparent resin layer on the film (the steps (1) and (2) above).
- This film having the transparent resin layer may be wound up once.
- the transparent film having the transparent resin layer 4b is subjected to rubbing treatment using a rubbing machine to impart orientation property to the transparent resin layer, whereby an orientation layer is formed
- the rubbing machine comprises a rubbing roller 8, a guide roller 6 fixed on a roller stage and a dust-removing machine 7 attached to the rubbing roller. Subsequently, dust on a surface of the orientation layer is removed using a surface dust-removing machine 9 disposed in the vicinity of the rubbing machine (the step (3) above).
- the known rubbing machine may be employed.
- the continuous transparent film having the orientation layer 4c is moved using a driving roller toward a coating machine 10.
- a coating liquid of a discotic compound having liquid crystalline property in a solvent is coated on the orientation layer using the coating machine 10 to form a coated layer (the step (4) above).
- the solvent in the coated layer is vaporized (the step (5) above), and the coated layer is heated to form a discotic nematic phase in a heating zone 11, whereby a layer of discotic compound having discotic nematic phase is formed (the step (6) above).
- the layer of discotic compound is exposed to ultraviolet light (UV light) emitted by UV lamp 12, to form a cured layer (the step (7) above).
- a polymerizable discotic compound i.e., a discotic compound having cross-linking groups
- the layer of discotic compound is cooled after heating for forming discotic nematic phase.
- the layer of discotic compound is generally cooled rapidly so as not to destroy the discotic nematic phase.
- the transparent film having the orientation layer and the layer of discotic compound generally are checked as to if the film is acceptable on not.
- the optical characteristics of the transparent film is measured by a device 13 for check, whereby the orientation condition of the layer of discotic compound is checked.
- the check is conducted by continuously measuring the optical characteristics of the transparent film.
- a protective film 14 is superposed on the transparent film having the orientation layer and the layer of discotic compound using a laminator 15 in such a manner that the protective film is in contact with the layer of discotic compound to form a composite film, and the composite film is wound up by a wind-up machine 16 (the step (8) above).
- the continuous optical compensatory sheet can be continuously prepared as shown in FIG. 2.
- FIG. 2 schematically shows another example of the process for the preparation of the continuous optical compensatory sheet of the invention.
- the continuous transparent film having a transparent resin layer (for forming an orientation layer) 4b is fed from a roll of the continuous film 5b using a delivery machine 1b, and driven using a driving roller.
- the steps of from the step of rubbing treatment to the step of winding up, which are performed after the above step, can be performed in the same manner as the steps explained as above referring to FIG. 1.
- the known delivery machines for feeding plastic film are employable.
- the known delivery machines include delivery machines utilizing superposition system (e.g., available from EAGAN Co., Ltd. and BLACK LOHSON Co., Ltd.), and seaming machines and unwinding machines used together with the seaming machines described in Japanese Patent Publication No. 48(1973)-38461.
- a shaftless turret unwinder is generally employed.
- an unwind side-guiding system used in unwinding (feeding) or winding roll stand e.g., those shown in COATING AND LAMINATING MACHINE, page 446, FIGS. 352A and 352B) can be employed.
- a lateral direction guiding machine using diaxial roll (Kamber roll) (e.g., one shown in COATING AND LAMINATING MACHINE, page 448, FIG. 355A) is generally employed after a drying zone (e.g., zone arranged after coating of coating liquid for forming transparent resin layer or layer of discotic compound), and a lateral direction guiding machine using a box roller (e.g., one shown in COATING AND LAMINATING MACHINE, page 448, FIG. 355B) is generally employed during movement of the film by the use of roller.
- Kamber roll e.g., one shown in COATING AND LAMINATING MACHINE, page 448, FIG. 355A
- a box roller e.g., one shown in COATING AND LAMINATING MACHINE, page 448, FIG. 355B
- a drum having a number of pores for suction can be employed as a driving machine for moving the film.
- edge winding system using a combination of saw blade cutting and adhesive (referring to catalog of EAGAN Co., Ltd. or Black Lohson Co., Ltd. describing turret winders) can be utilized.
- edge winding system using a combination of saw blade cutting and adhesive referring to catalog of EAGAN Co., Ltd. or Black Lohson Co., Ltd. describing turret winders
- the above shaftless turret unwinder is generally employed, and the above unwind side guiding system can be also employed.
- the step of forming the transparent resin layer for forming an orientation layer (the step (2) above) is explained referring to FIG. 3.
- the step can be, for example, performed below.
- a coating liquid containing a resin for forming an orientation layer in a coating liquid tank 31 is fed, using a pump 32, through a filter 33 to inside of an extrusion die 35 having a vacuum chamber 35a.
- the coating liquid is coated on a surface of a moving transparent film 34 (corresponding to 4a of FIG. 1) by the extrusion die while the transparent film is supported by a back-up roller 36.
- the number 39 is an air fan.
- the transparent film having the coated layer is moved in a transporting zone 37 for initial drying, passed through the zone, and then dried in a drying zone 38.
- the dried film is continuously subjected to the next rubbing treatment, or is once wound up.
- a gap between the edge of the extrusion die 35 and the transparent film 34 is generally in the range of 100 to 300 ⁇ m.
- the vacuum chamber 35a is kept at a pressure lower by 200 to 500 Pa than the atmospheric pressure.
- the rate of movement of the transparent film (coating rate) preferably is in the range of 0.1 to 1.0 m/sec.
- the drying in the drying zone preferably is at a temperature of 50° to 100° C. (especially 70° to 100° C.) and preferably is for a time period of 1 to 10 min.
- the coating liquid preferably has a viscosity of 1 to 20 mPa.s, and the coated amount preferably is in the range of 10 to 50 g/m 2 .
- the coating can be performed using a wire-bar instead of the extrusion die, the wire-bar being used in the forming of a layer of discotic compound described later.
- FIG. 4 The section view of the extrusion die employed above is shown in FIG. 4.
- an extrusion die 41 having a manifold 41a and a slot 41b is mounted on a trestle 42 provided with a vacuum chamber 43 having a discharge opening 44 and an exhaust vent 45.
- the coating liquid is fed into the manifold 41a and coated through the slot 41b on the moving transparent film which is supported by a back-up roller 46.
- An angle of the direction of the slot of the extrusion die 41 from the horizon preferably is in the range of 30 to 50 degrees.
- the edge of the extrusion die 41 is preferably disposed such that the angle of a line combining the edge with the center of the back-up roller from the horizon is in the range of ⁇ 5 degrees.
- FIG. 5(A) shows a plan view of a rubbing machine
- FIG. 5(B) shows a section view of the rubbing machine.
- the transparent film having the transparent resin layer 54 (corresponding to 5b of FIG. 1) is moved in the direction of an arrow, and a surface of the transparent resin layer is rubbed by a rubbing roller (e.g., one having outer diameter of 150 mm) 58 rotating in the reverse direction of the moving direction, while the upper side of the film on the rubbing roller is depressed by a guide roller 56 attached to a roller stage 53.
- a rubbing sheet such as velvet 58a is wound around the rubbing roller 58, and the rubbing sheet directly rubs the surface of the transparent resin layer.
- the rubbing roller 58 is rotated by a motor M.
- the rate of rotation of the rubbing roller can be adjusted in the range of less than approx. 1,000 rpm, and the rubbing roller can be appropriately rotated with respect to horizontal against the moving direction to obtain an desired rubbing angle.
- the rubbing roller is rotated, taking as an axial a position showing a center of the length of the rubbing roller, to adjust a rubbing angle, and under this condition, the transparent film is moved at a constant tension and a constant rate (generally a rate of not less than 5 m/min.) while the rubbing roller is rotated at a constant rate of revolution in the reverse direction against the moving direction of the film, whereby the rubbing can be continuously performed.
- a constant tension and a constant rate generally a rate of not less than 5 m/min.
- the film can be moved with floating by an airfoil effect, and therefore the film is scarcely shifted in the width direction and thus the continues rubbing of the film can be stably performed.
- the guide roller 56 is provided with a mechanism detecting the tension of the film whereby the tension of the film during rubbing can be controlled. Moreover, the guide roller can move vertically the rubbing roller to enable adjustment of a lap angle.
- the outer diameter of the rubbing roller generally is in the range of 80 to 500 mm, preferably in the range of 100 to 200 mm.
- the rotation number of the rubbing roller generally is in the range of 500 to 1,500 r.p.m.
- a base lap angle preferably is in the range of 4 to 20 degrees, and the tension of the film preferably is in the range of 1 to 2N/1 cm (1:film width).
- the rubbing roller is generally used in combination of two to four rollers.
- the rotating axis of the rubbing roller can be generally adjusted in the range of 0 to 45 degrees. Further, it is preferred that the rubbing roller can be attached or removed at the joining area by a machine moving vertically the rubbing roller.
- the rate of movement of the film generally 6 to 60 m/min. as mentioned previously (preferably 10 to 50 m/min.).
- Dust on the surface of the rubbing sheet 58a of the rubbing roller 58 is removed using a dust-removing machine 57 disposed in the vicinity of the side of the rubbing roller 58 immediately after the film is rubbed. Therefore, dust produced during the rubbing of the film scarcely remains on the surface of the rubbing sheet 58a, and naturally dust on the rubbing sheet scarcely migrates into the surface of the film. In the dust-removing machine 57, an air AR is introduced and discharged.
- Both the surface of the rubbed transparent resin layer (i.e., orientation layer) and the surface having no resin layer of the transparent film are destaticized using a static eliminator 55. Subsequently, dust on the surface of the orientation layer is removed by a dust-removing machine 59a disposed in the vicinity of the back-up roller 52a, and dust of the surface having no orientation layer of the film is removed by a dust-removing machine 59b disposed in the vicinity of the back-up roller 52b. In the step for removal of dust, dust of the surface of orientation layer only may be removed.
- an ultrasonic dust-removing machine is preferred.
- the machine has function of blowing compressed air with supersonic vibration and sucking produced dust.
- trade names of the machine include New Ultra Cleaner (UVU-W type; available from Koshin Co., Ltd.).
- a rate of blowing air generated by the ultrasonic dust-removing machine generally is in the range of 10 to 50 m/sec., preferably in the range of 10 to 30 m/sec.
- a distance between the surface of the roller and the edge of the dust-removing machine preferably is in the range of 2 to 5 mm.
- the removal of dust from the orientation layer can be also conducted using the device as shown in FIG. 6.
- a solvent is sprayed using a spray coater 61, and immediately (before the solvent vaporizes) the solvent on the orientation layer is scraped together with dust by rotating a roller for scraping 63 in the reverse direction to the moving direction of the film with depressing the film by a guide roller 62. Thereafter, the film is dried (generally at a temperature of 40° to 70° C.) in a drying chamber 65.
- the spray coater a coater in which nozzles having a diameter of 1 mm are disposed at interval of 3 mm in the form of hound's-tooth check can be employed.
- the roller for scraping generally has a diameter of 2 to 30 mm, preferably 5 to 30 mm.
- dust-removing devices by spray of solvent described above, dust-removing devices described in Japanese Patent Provisional Publication No. 62(1987)-60750 (e.g., methods shown in FIGS. 1 and 3) can be utilized.
- the removal of dust from the orientation layer or on the transparent film can be conducted by using the device as shown in FIG. 7.
- Both of the surface of the orientation layer and the surface having no resin layer of the moving transparent film 74, are destaticized using a static eliminator 75.
- the transparent film is passed through between a back-up roller 72a and a roller having an adsorptive layer 79a thereon which is disposed facing to the back-up roller 72a, whereby dust on the surface of the orientation layer is removed by allowing the dust to migrate from the surface of the orientation layer to the surface of the adsorptive layer.
- the transparent film is passed through between a back-up roller 72b and a roller having an adsorptive layer 79b which is disposed facing to the back-up roller 72b, whereby dust on the reverse surface of the transparent film is removed. In the removal of dust, only dust on the surface of orientation layer may be removed.
- materials of the adsorptive layer include silicone rubber, polyurethane rubber, acrylic rubber and nitrile rubber.
- Any method of rubbing treatment other than the method described above can be utilized in the invention, so long as the continuous (or longitudinal) film can be continuously rubbed.
- a back-up rubbing method wherein a rubbing roller depresses a continuous film under running at the position of a back-up roller (pass roller) supporting the film, described in Japanese Patent Provisional Publication No. 61(1986)-160720, and a lap rubbing method wherein a rubbing roller depresses a continuous film at the position between two back-up rollers supporting the film, and another back-up rubbing method wherein a rubbing roller depresses a continuous film with supporting the film by sprockets disposed at both ends of the rubbing roller, described in Japanese Patent Provisional Publication No. 6(1994)-110059.
- a cleaning tape may be moved in the rubbing machine to remove dust attached to rollers in the machine.
- FIG. 8 shows a plan view of a wire-bar coating machine
- FIG. 9 shows a section view of a wire-bar coating machine.
- a wire-bar 81 is supported at both edges by bearings 83, and a coating liquid falling from the wire-bar is received by an interstructure (wall) 82 which is disposed under the wire-bar.
- the both edges of the wire-bar are combined to a motor 85 through a coupling 84.
- a coating liquid containing a discotic compound supplied at a feed opening 89A is fed into a primary liquid well 86, and into a secondary liquid well 87 through a connecting pipe 96 passing through the interstructure 82.
- Liquid levels of the coating liquid in the primary liquid well 86 and the secondary liquid well 87 are controlled by a regulating plate 92, and overflowing coating liquid is discharged from a discharge opening 89B through an overflowing liquid well 88.
- the coating liquid may be fed to the secondary liquid well while coating is conducted.
- provision of the connecting pipe is preferred to keep uniformity of the coating liquid.
- the discharged coating liquid is adjusted to an appropriate viscosity by adding a solvent in a viscosity-control chamber 95, and is continuously filtered with a filter 93 with being fed by a pump 97 to be fed to the feed opening 89A again.
- the viscosity of the coating liquid is adjusted based on the density which is measured by a density instrument 98 disposed before the filter 93.
- the coating liquid discharged at the discharge opening 89B is fed through an inlet 107 to a coating liquid tank 102 which is filled with an amount of coating liquid.
- the coating liquid in the coating liquid tank 102 is controlled so as to have an appropriate viscosity, and thus the coating liquid having the controlled viscosity, which has the same amount as the coating liquid fed through the inlet 107, is fed through an outlet 108 to the feed opening 89A of the wire-bar coating machine.
- a density of a coating liquid fed through the outlet 108 of viscosity-control chamber 95 is measured by the density instrument 98 of FIG. 9, and the value of density is input to a control unit 106 to control an air pressure unit 105, whereby a solvent (e.g., methyl ethyl ketone) in a solvent tank 104 is fed using a dosing bulb 103 to the coating liquid tank 102 such that the coating liquid has an appropriate viscosity. Further, the coating liquid in the coating liquid tank 102 is always stirred by a rotor blade 109b driven by a motor 109a to form a homogeneous phase.
- a solvent e.g., methyl ethyl ketone
- the coating is performed by continuously bringing an orientation layer of a moving continuous transparent film having the orientation layer 94a into contact with a surface of the wire-bar 81 under rotation to which the coating liquid having the above controlled viscosity adheres.
- the coating liquid lifted up from the primary liquid well 86 by rotating the wire-bar in the same direction as that of the film 94a and at the almost same rate as that of the film 94a is brought into contact with the orientation layer of the transparent film 94a to give a transparent film having a coated layer 94b.
- the rotation rate of the wire-bar is preferably a rate of 0.8 to 1.2 times the rate of movement of the film.
- the coating liquid in the primary liquid well of wire-bar coating machine preferably has a residence (retention) time of not more than 10 seconds, especially not more than 9 seconds.
- the lower limit generally is 0.2 seconds.
- the residence time (T) is defined by the formula:
- V 1 represents a volume (cm 3 ) of the primary liquid well
- Q represents a cycling flow rate (cm 3 /sec.).
- the wire-bar 61 is allowed to have its surface higher by 20 mm or more than the location at which the wire-bar is positioned when the coating is not performed.
- the coating liquid preferably contains the discotic compound in an amount of 15 to 50 weight %, especially in an amount of 15 to 40 weight %.
- the viscosity of the coating liquid preferably is in the range of 1 to 20 mpa.s at 25° C., especially 1 to 15 mpa.s.
- the coating is generally performed at a temperature of 10° to 40° C.
- wire-bar coating machines other than the above machine, there can be employed those described in Japanese Patent Publication No. 58(1983)-4589.
- a coating liquid of a discotic liquid crystalline compound in a solvent is coated using a bar coater 111 as described above.
- the transparent film having the coated layer of discotic compound 114b is moved along a rectifiable plate 112 to a drying zone 116, and then moved to a heating zone 119.
- a time period of from a few seconds to a few minutes after the coating corresponds to that showing a constant rate drying speed in which the reducing rate (speed) of the solvent in the coated layer is proportional to time.
- the constant rate drying speed is described in "Chemical Engineering Handbook" (pp.707-712, Edited by Maruzen Co., Ltd., Oct. 25, 1980).
- the inventor found that when, in the time period, wind or heating is nonuniformly applied to the coated layer, a thickness of the coated layer is rendered uneven, whereby nonuniformity of oriented conditions of the layer is produced.
- This problem is solved by the process of vaporizing the solvent from the coated layer under sealing the coated layer with a gaseous layer (i.e., drying of the coated layer is conducted so as to scarcely apply wind to the coated layer before heating).
- a gas for drying is introduced into the drying zone 116 through a metallic netting 115a from an intake vent 113a.
- the gas introduced from an intake vent 113a is discharged at an exhaust vent 113b, and at the same time passed through the metallic netting 115a, a porous plate 118 and a metallic netting 115b to be discharged at a second exhaust vent 117.
- the provision of these porous plate 118 and a metallic netting 115b scarcely brings about marked variation of rate or direction of air.
- An interval between the rectifiable plate 112 and the transparent film preferably is in the range of 1 to 10 mm.
- the length of the rectifiable plate preferably is in the range of 1 to 5 m.
- the rate of gas at the metallic netting 115a generally is approx. 0.3 m/sec.
- the temperature generally is in the range of room temperature to 50° C., preferably 20° to 50° C.
- the running rate of the support generally is in the range of 6 to 60 m/min. (preferably in the range of 5 to 30 m/min.).
- the length of the drying zone 116 generally is in the range of 0.5 to 10 m.
- the sealing of the gaseous layer can be conducted by moving the gaseous layer at a relative rate of -0.1 to 0.1 m/sec. to the movement rate of the coated layer.
- the transparent film having the coated layer subjected to the drying treatment is subsequently heated.
- the step of heating the coated layer to form a discotic nematic phase (the step (6) above) is explained referring to FIG. 11.
- heated air which is introduced from air plenums 119a, 119b provided on both sides of the transparent film, is blown on both sides of the transparent film having the coated layer.
- the heated air is generally set to have a temperature of 70° to 300° C.
- Examples of means for heating other than heated air include application of far infra-red rays and interaction of heated roll.
- the obtained layer of discotic compound is cooled (the step (7) above).
- the transparent film having the layer of discotic compound is rapidly cooled by applying an air to the film or bringing the film into contact with a cooled roll, whereby the solidified layer of discotic compound can be obtained.
- the obtained layer of discotic compound is continuously subjected to light (preferably UV light) irradiation treatment (the step (7) above) without cooling. This step is explained referring to FIGS. 12 and 13.
- the transparent film having the layer of discotic compound 124 is moved to an ultraviolet-light irradiation device 123 (generally having a permeable sheet to UV light mainly shielding cooled air) which is provided in the vicinity of the above heating zone to be passed through it, whereby the layer of discotic compound is exposed to UV light to be polymerized (cured). Subsequently, the transparent film having the orientation layer and the layer of discotic compound is wound up, or laminated with a protective film and then wound up (the step (8) above).
- an ultraviolet-light irradiation device 123 generally having a permeable sheet to UV light mainly shielding cooled air
- the ultraviolet-light irradiation device 123 has an ultraviolet lamp 121 and a transparent plate 122 which UV light is passed through and shields heat rays and wind.
- An air for cooling is given around the ultraviolet lamp 121 using an air fan for cooling a lamp 126.
- the transparent film having the layer of discotic compound 134 is moved to an ultraviolet-light irradiation device 133 (generally having a permeable sheet to UV light mainly shielding cooled air) disposed over a roller 132, and passed through the ultraviolet-light irradiation device 133 such that the film is supported around the roller 132, whereby the layer of discotic compound is exposed to UV light to be polymerized (cured). Subsequently, the transparent film having the orientation layer and the layer of discotic compound is wound up, or laminated with a protective film and then wound up.
- an ultraviolet-light irradiation device 133 generally having a permeable sheet to UV light mainly shielding cooled air
- the process of the invention is suitable for a process for industrial preparation of the sheet or for mass production of the sheet.
- the continuous optical compensatory sheet obtained by the process of the invention has a uniformly oriented discotic compound layer almost free from adhesion of dust and occurrence of shifting of film which gives occurrence of variation of a thickness of the sheet. Therefore, the process of the invention enables preparation in high productivity of the continuous optical compensatory sheet which gives a liquid crystal display almost free from variation of image. Thus, the process enables mass production of the continuous optical compensatory sheet having good characteristics.
- the optical compensatory sheet of the invention is basically composed of a transparent film, the orientation layer thereon and the layer of discotic compound (also referred to as optically anisotropic layer).
- any material can be employed so long as it is transparent.
- the material preferably has a transmittance of not less than 80% and specially shows optical isotropy when it is viewed from a front side.
- the film preferably has a negative uniaxial property and an optic axis in the normal line direction.
- the film is preferably prepared from materials having a small intrinsic birefringence, such as triacetyl cellulose.
- materials having a small intrinsic birefringence such as triacetyl cellulose.
- Such material is available on market by the trade name of Geonex (from Nippon Geon Co., Ltd.), Arton (from Japan Synthetic Rubber Co., Ltd.) or Fuji TAC (from Fuji Photo Film Co., Ltd.).
- materials having a large intrinsic birefringence such as polycarbonate, polyallylate, polysulfone and polyethersulfone can be also employed by rendering the materials optically isotropic by appropriately controlling molecular orientation in a procedure of forming a film.
- the transparent film generally satisfies the condition of:
- nz ⁇ nx ny (i.e., negative uniaxial property) and preferably satisfies the condition of:
- nx and ny are main refractive indices within the film and nz is a main refractive index in a thickness direction of the film, and more preferably satisfies the condition of:
- the transparent film preferably satisfies the condition of:
- nx and ny have the same meanings as above and d is a depth (i.e., thickness) direction of the film.
- ⁇ d of retardation from front side (when the display is viewed from the front side) preferably is not more than 50 nm, especially not more than 20 nm.
- the orientation layer is generally provided on the transparent film.
- the orientation layer has a function of defining an orientation direction of a discotic liquid crystalline compound to be provided thereon by a coating method, and the orientation gives an optic axis inclined from an optical compensatory sheet.
- any layers can be employed so long as they are capable of imparting orientation property to an optically anisotropic layer (layer of discotic compound).
- a layer of an organic compound (preferably polymer) subjected to rubbing treatment is employed.
- orientation layer examples include polymers such as polymethyl methacrylate, acrylic acid/methacrylic acid copolymer, styrene/maleinimide copolymer, polyvinyl alcohol, poly(N-methylolacrylamide), styrene/vinyltoluene copolymer, chlorosulfonated polyethylene, nitrocellulose, polyvinyl chloride, chlorinated polyolefin, polyester, polyimide, vinyl acetate/vinyl chloride copolymer, ethylene/vinyl acetate copolymer, polyethylene, polypropylene, and polycarbonate; and organic substances such as saline coupling agents.
- polymers such as polymethyl methacrylate, acrylic acid/methacrylic acid copolymer, styrene/maleinimide copolymer, polyvinyl alcohol, poly(N-methylolacrylamide), styrene/vinyltoluene copolymer, chlorosulf
- polymers for the orientation layer include polyimide, polystyrene, polymer of styrene derivatives, gelatin, polyvinyl alcohol and polyvinyl alcohol having an alkyl group (preferably having 6 or more carbon atoms).
- Orientation layers obtained by subjecting films of these polymers to orientation treatment are capable of tilting obliquely discotic liquid crystalline compound.
- the polyvinyl alcohol or modified polyvinyl alcohol generally has saponification degree in the range of 70 to 100%, preferably in the range of 80 to 100%, and especially in the range of 85 to 95%.
- a polymerization degree of the above polyvinyl alcohol or modified polyvinyl alcohol preferably is in the range of 100 to 3,000.
- modified polyvinyl alcohols include polyvinyl alcohols modified by copolymerization having a group such as --COONa, --Si(OX) 3 X: hydrogen or halogen!, --N(CH 3 ) 3 .Cl, C 9 H 19 COO--,--SO 3 Na or --C 12 H 25 ; polyvinyl alcohols modified by incorporation of chain-transfer agent employed in copolymerization having a terminated group such as --COONa, --SH or C 12 H 25 S--; and polyvinyl alcohols modified by block-copolymerization having a group such as --COOH, --CONH 2 ,--COOR R: alkyl! or C 6 H 5 --.
- the modified polyvinyl alcohol preferably is a polymer obtained by reacting polyvinyl alcohol with a compound of the formula (1): ##STR1## in which R 1 represents an alkyl group or an alkyl group substituted with alkyl, acryloyl, methacryloyl or oxiranyl; W represents a halogen atom, an alkyl group or an alkoxy group; X represents an atomic group for forming active ester, acid anhydride or acyl halide together with --CO--; 1 is 0 or 1; and n is an integer of 0 to 4.
- the alkyl group of R 1 preferably has 2 to 24 carbon atoms, and the alkyl group and alkoxy group of W preferably have 2 to 24 carbon atoms.
- the formula (I) preferably is in the form of the following formula (2): ##STR2## in which X 1 represents an atomic group for forming active ester, acid anhydride or acyl halide together with --CO--; and m is an integer of 2 to 24.
- polyvinyl alcohols to be employed to react with the compound of the formula (1) or (2) include polyvinyl alcohols and modified polyvinyl alcohols described above (i.e., polyvinyl alcohols modified by copolymerization, polyvinyl alcohols modified by incorporation of chain-transfer agent; and polyvinyl alcohols modified by block-copolymerization).
- a polyimide film (preferably fluorine-containing polyimide film), which is widely used as an orientation layer for a liquid crystal cell, is also preferably employed as the orientation layer of the invention.
- the polyimide film can be prepared by coating a solution of polyamic (polyamide) acid (e.g., a series of LQ/LX available from Hitachi Chemical Co., Ltd.; and a series of SE available from Nissan Chemical Industries, Ltd.) on the transparent film, dried (burned) at 100° to 300° C. for 0.5 to 1 hour, and rubbing a surface of the resultant polyimide film.
- polyamic (polyamide) acid e.g., a series of LQ/LX available from Hitachi Chemical Co., Ltd.; and a series of SE available from Nissan Chemical Industries, Ltd.
- the orientation layer for the discotic liquid crystalline compound can be prepared by rubbing the transparent resin layer (polymer layer) in the known manner which is conventionally employed to prepare an orientation layer or surface for liquid crystal of LCD.
- the treatment is performed to give a function of orienting a liquid crystal to a surface of the orientation layer by rubbing the surface in a certain direction by the use of paper; gauze; felt; a sheet made of rubber, polyamide (nylon) or polyester; or a sheet made of fiber of polyamide (nylon), layon or polyester (e.g., velvet).
- a relative rate of the sheet to the orientation layer generally is in the range of 50 to 1,000 m/min., preferably in the range of 100 to 500 m/min.
- the layer of discotic compound (optically anisotropic layer) having discotic nematic phase is formed on the orientation layer.
- the layer of discotic compound is obtained by orienting the coated layer of discotic compound and cooling, or by orienting the coated layer of discotic compound having polymerizable group and curing, and the layer of discotic compound has a negative birefringence.
- Examples of the compounds include benzene derivatives described in C. Destrade et al., Mol. Cryst. vol. 71, pp. 111, 1981, truxene derivatives described in C. Destrade et al., Mol Cryst. vol. 122, pp. 141. 1985, Physics lett. A, vol. 78, pp. 82, 1990, cyclohexane derivatives described in B. Kohn et al., Angew. Chem. vol. 96, pp. 70, 1984, macrocyclic compounds of azacrown-type or phenylacetylene-type described in J. M. Lehn et al., J. Chem. Commun. pp.
- the discotic liquid crystal generally has a structure that the above compound is located at a center of the crystal as a parent core and further straight chain groups such as alkyl, alkoxy and benzoyl having a substituent are radially bonded to the compound.
- any discotic liquid crystalline compounds can be used, so long as the liquid crystals have a negative birefringence (negative uniaxial property) and orientation property.
- the layer of discotic compound can be prepared by coating a solution of the discotic compound (and other compound if desired) in a solvent on the orientation layer, dried, heating to temperature for forming a discotic nematic phase and cooling with keeping the oriented condition (discotic nematic phase). Otherwise, the layer can be prepared by coating a solution of a polymerizable discotic compound (and other compound if desired) in a solvent on the orientation layer, dried, heating to temperature for forming a discotic nematic phase, polymerizing the coated layer (e.g., by radiation of UV light) and cooling.
- the transition temperature of from discotic nematic phase to solid phase generally is in the range of 70° to 300° C., preferably in the range of 70° to 170° C.
- the inclined angle of the discotic unit on the support side can be generally controlled by selection of discotic compounds or materials of the orientation layer, or selection of methods for rubbing treatment.
- the inclined angle of the discotic unit on a surface side (air side) can be controlled by selection of discotic compounds or other compounds (e.g., plasticizer, surface active agent, polymerizable monomer and polymer) employed together with the discotic liquid crystalline compound.
- the extent of variation of the inclined angle can be also controlled by the above selection.
- any compounds can be employed so long as they are compatible with the discotic compound and have properties of giving the inclined angle of the discotic liquid crystalline compound or not inhibiting orientation of the discotic liquid crystalline compound.
- Preferred is polymerizable monomer (e.g., compounds having a vinyl, vinyloxy, acryloyl or methacryloyl group).
- the compound are preferably used in the amount of 1 to 50 weight % (especially 5 to 30 weight %) based on the amount of the discotic compound.
- any polymers can be employed, so long as they are compatible with the discotic compound and are capable of giving the inclined angle of the discotic liquid crystalline compound.
- the polymer are generally used in the amount of 0.1 to 10 weight % (preferably 0.1 to 8.0 weight % and especially 0.1 to 5.0 weight %) based on the amount of the discotic compound, so as not to inhibit orientation of the discotic liquid crystalline compound.
- the optical compensatory sheet obtained by the process of the invention generally has the minimum absolute retardation value in a direction inclined from the normal of the sheet and has no optic axis.
- the representative structure of the optical compensatory sheet containing the optically anisotropic layer is shown in FIG. 14.
- a transparent film 141, an orientation layer 142 and a layer of discotic compound 143 are superposed in order to constitute the optical compensatory sheet.
- the reference number R indicates the rubbing direction of the orientation layer.
- n 1 , n 2 and n 3 indicate refractive indices in the three axes direction of the optical compensatory sheet, and n 1 , n 2 and n 3 satisfy the condition of n 1 ⁇ n 3 ⁇ n 2 , in the case that are seen in the front direction.
- the reference number ⁇ is an inclined angle of the direction showing the minimum of Re from the normal 144 of the optically anisotropic layer.
- the direction showing the minimum retardation value of the optically anisotropic layer is preferably inclined at 5 to 50 degrees from a normal line of the sheet ( ⁇ in FIG. 4) and especially 10 to 40 degrees.
- the sheet satisfies the condition of:
- D is a thickness of the sheet
- the solution for forming the layer of discotic compound is generally prepared by dissolving the discotic compound(s) and other compounds described previously in a solvent.
- solvents employable for dissolving the compound therein include polar solvents such as N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO) and pyridine, nonpolar solvents such as benzene and hexane, alkyl halides such as chloroform and dichloromethane, esters such as methyl acetate and butyl acetate, ketones such as acetone and methyl ethyl ketone, and ethers such tetrahydrofuran and 1,2-dimethoxyethane. Preferred are alkyl halides and ketones.
- the solvents may be employed singly or in combination.
- the coating the above solution thereof is conducted using wire-bar coating machine as described previously.
- FIG. 15 The representative structure of the liquid crystal display having the above optical compensatory sheet obtained by the invention is shown in FIG. 15.
- a liquid crystal cell TNC comprising a pair of substrates provided with a transparent electrode and a twist-oriented nematic liquid crystal sealed therebetween, a pair of polarizing plates A and B arranged on the both sides of the cell, the optical compensatory sheets RF 1 and RF 2 between the liquid crystal cell and the polarizing sheet and back light BL are assembled to constitute the liquid crystal display.
- the optical compensatory sheet may be arranged only on one side (i.e., use of one of RF 1 and RF 2 ).
- the reference number R 1 is a rubbing direction of the orientation layer of the optical compensatory sheet RF 1
- the reference number R 2 is the rubbing direction of the orientation layer of the optical compensatory sheet RF 2 , in the case that are seen in the front direction.
- An arrow of a solid line of the liquid crystal cell TNC indicates the rubbing direction of the polarizing sheet B side substrate of TNC
- an arrow of a dotted line of the liquid crystal cell TNC indicates the rubbing direction of the polarizing sheet A side substrate of TNC.
- PA and PB are polarizing axes of polarizing sheets A and B, respectively.
- optical compensatory sheet was prepared according to the continues steps of from a step of feeding a continuous transparent film to a step of winding up a resultant continuous optical compensatory sheet as shown in FIG. 1.
- a coating liquid for forming an orientation layer 5 weight % aqueous solution of polyvinyl alcohol having long chain alkyl groups (MP-203, produced by Kuraray Co., Ltd.)! was coated.
- the coating was conducted with moving the triacetyl cellulose film at a rate of 20 m/min., and then dried by passing the film through a drying zone (temperature: 90° C.; length: 80 m) with moving the film at the same rate, to form a trans-parent resin layer having a thickness of 2.0 ⁇ m (film 4b in FIG. 1 was obtained).
- the formation of the transparent resin layer was conducted using the coating machine and drying machine shown in FIG. 3.
- the surface of the resultant transparent resin layer was subjected to rubbing treatment with moving the triacetyl cellulose film at a speed of 20 m/min.
- the rubbing treatment was conducted using the rubbing machine shown in FIG. 5 in the conditions of the number of revolution of the rubbing roller 58 of 300 rpm, whereby an orientation layer was formed. Thereafter dust of the orientation layer was removed.
- the following coating liquid for forming layer of discotic compound was continuously coated in a coating amount of 5 cc/m 2 on the orientation layer by the use of an wire-bar coating machine 10 (FIG. 1), with moving the triacetyl cellulose film having the orientation layer 4c (FIG. 1) at a speed of 20 m/min.
- the wire-bar coating machine the machine shown in FIGS. 8 and 9 was employed.
- the triacetyl cellulose film having the coated layer was passed through a drying zone 116 shown in FIG. 11 at a rate of movement of 20 m/min. to dry the coated layer, and continuously the coated layer was passed through a heating zone 119 for orientation shown in FIG. 11 to orient the discotic compound.
- the drying zone 116 Wind velocity of 0.1 m/sec., was introduced from a metallic netting 115a.
- the heating zone 119 was set to have a temperature of 130° C.
- the film having the coated layer was entered in the drying zone after 3 seconds from completion of the coating and passed through for 3 seconds. Immediately, the film having the coated layer was entered in the heating zone and was passed through the heating zone for approx. 3 minutes.
- the transparent film having the coated layer was passed through a UV zone 12 at a rate of movement of 20 m/min.
- the coated layer was exposed to UV light (a high-pressure mercury lamp (out-put power: 160 W/cm, emission length: 1.6 m)) in intensity of illumination of 600 mW/cm 2 for four seconds by the use of the UV irradiation device shown in FIG. 12, to cure the coated layer, and cooled to room temperature to form a layer of discotic layer.
- the film having the orientation layer and the layer of discotic compound was checked by measuring the optical characteristics of the film by the use of a device for check 13 (FIG. 1) with moving the film at a speed of 20 m/min. Then, a protective film 14 (FIG. 1) was superposed on the layer of discotic compound of the film using a laminator 15 (FIG. 1), and wound up by a winding machine. Thus, a continuous optical compensatory sheet in the form of roll, which comprises a transparent film, an orientation layer and a layer of discotic compound, was obtained.
- Example 1 The procedures of Example 1 were repeated except for changing the number of revolution of the rubbing roller 58 in the rubbing treatment from 300 rpm to 500 rpm, to prepare a continuous optical compensatory sheet.
- Example 1 The procedures of Example 1 were repeated except for changing the number of revolution of the rubbing roller 58 in the rubbing treatment from 300 rpm to 700 rpm, to prepare a continuous optical compensatory sheet.
- Example 1 The procedures of Example 1 were repeated except for changing the number of revolution of the rubbing roller 58 in the rubbing treatment from 300 rpm to 900 rpm, to prepare a continuous optical compensatory sheet.
- Example 1 Employing the materials and machines of Example 1, a wound optical compensatory sheet was prepared in a batch production instead of continuous production.
- the continuous optical compensatory sheet was observed using a polarizing microscope (performed in the check step using device for check 13 (FIG. 1)). In more detail, occurrence of schlieren or columnar phase of the optical compensatory sheet, which shows nonuniform orientation, was observed.
- optical compensatory sheet was prepared according to the continues steps of from a step of feeding a continuous transparent film to a step of winding up a resultant continuous optical compensatory sheet as shown in FIG. 1.
- a coating liquid for forming an orientation layer 5 weight % aqueous solution of polyvinyl alcohol having long chain alkyl groups (MP-203, produced by Kuraray Co., Ltd.)! was coated.
- the coating was conducted with moving the triacetyl cellulose film at a rate of 20 m/min., and then dried by passing the film through a drying zone (temperature: 90° C., length: 80 m) with moving the film at the same rate, to form a transparent resin layer having a thickness of 2.0 ⁇ m (film 4b in FIG. 1 was obtained).
- the formation of the transparent resin layer was conducted using the coating machine and drying machine shown in FIG. 3.
- the surface of the resultant transparent resin layer was subjected to rubbing treatment with moving the triacetyl cellulose film at a speed of 20 m/min.
- the rubbing treatment and dust-removing treatment was conducted using the rubbing machine shown in FIG. 5.
- the transparent film having the transparent resin layer 54 was moved in the direction of an arrow at a speed of 20 m/min., and a surface of the transparent resin layer was rubbed by a rubbing roller (outer diameter: 150 mm) 58 rotating at 600 rpm in the reverse direction of the moving direction of the film, while the upper side of the film on the rubbing roller was depressed by a guide roller (outer diameter: 65 mm) 56 attached to a roller stage 53.
- a rubbing sheet of velvet 58a was wound around the rubbing roller, and therefore the rubbing sheet directly rubbed the surface of the transparent resin layer.
- the rubbing was conducted in the conditions of the base lap angle of 6 degrees, the tension of the film of 1.8N/1 cm (1:film width) and the rotating axis of the rubbing roller to the width direction of 0 degree.
- both the surface of the rubbed transparent resin layer (i.e., orientation layer) and the surface having no resin layer of the transparent film were destaticized using a static eliminator 55, and then dust on the surface of the orientation layer was removed by a dust-removing machine 59a disposed in the vicinity of the back-up roller (diameter: 100 mm) 52a, and dust on the surface having no orientation layer of the film was removed by a dust-removing machine 59b disposed in the vicinity of the backup roller (diameter: 100 mm) 52b.
- the dust removal was conducted using as the dust-removing machine the ultrasonic dust-removing machine (New Ultra Cleaner (UVU-W type); available from Koshin Co., Ltd.) under the conditions of a head pressure of 3,000 mmAq, a rate of blowing air generated by the ultrasonic dust-removing machine of 20 m/sec. and a distance between the surface of the roller and the end of the ultrasonic dust-removing machine of 2 mm.
- the ultrasonic dust-removing machine New Ultra Cleaner (UVU-W type); available from Koshin Co., Ltd.
- a coating liquid for forming layer of discotic compound was continuously coated in a coating amount of 5 cc/m 2 on the orientation layer by the use of an wire-bar coating machine 10 (FIG. 1), with moving the triacetyl cellulose film having the orientation layer 4c (FIG. 1) at a speed of 20 m/min.
- the coating liquid for forming layer of discotic compound the same coating liquid as in Example 1 was employed.
- the wire-bar coating machine the machine shown in FIGS. 8 to 10 was employed.
- the triacetyl cellulose film having the coated layer was passed through a drying zone 116 shown in FIG. 11 at a rate of movement of 20 m/min. to dry the coated layer, and continuously the coated layer was passed through a heating zone 119 for orientation shown in FIG. 11 to orient the discotic compound.
- the drying zone 116 Wind velocity of 0.1 m/sec., was introduced from a metallic netting 115a.
- the heating zone 119 was set to have a temperature of 130° C.
- the film having the coated layer was entered in the drying zone after 3 seconds from completion of the coating and passed through for 3 seconds. Immediately, the film having the coated layer was entered in the heating zone and was passed through the heating zone for approx. 3 minutes.
- the transparent film having the coated layer was passed through a UV zone 12 (FIG. 1) at a rate of movement of 20 m/min.
- the coated layer was exposed to UV light (a high-pressure mercury lamp (out-put power: 160 W/cm, emission length: 1.6 m)) in an intensity of illumination of 600 mW/cm 2 for four seconds by the use of the UV irradiation device shown in FIG. 12, to cure the coated layer, and cooled to room temperature to form a cured layer of discotic layer.
- the film having the orientation layer and the layer of discotic compound was checked by measuring the optical characteristics of the film by the use of a device for check 13 (FIG. 1) with moving the film at a speed of 20 m/min. Then, a protective film 14 (FIG. 1) was superposed on the layer of discotic compound of the film using a laminator 15 (FIG. 1), and wound up by a winding machine. Thus, a continuous optical compensatory sheet in the form of roll, which comprises a transparent film, an orientation layer and a layer of discotic compound, was obtained.
- Example 5 The procedures of Example 5 were repeated except for performing the dust removing after the rubbing treatment using the device shown in FIG. 6 in the following manner, to prepare a continuous optical compensatory sheet.
- methyl ethyl ketone was sprayed in a spraying amount of 10 cc/m 2 using a spray coater 61, and immediately (after one second from the spraying) the solvent on the orientation layer was scraped together with dust by rotating a roller for scraping (outer diameter: 5 mm) 63 at 100 rpm in the reverse direction to the moving direction of the film with depressing the film by a guide roller 62. Thereafter, the film was dried in a drying chamber (at 60° C.) 65 for one minutes.
- a coater in which nozzles having a diameter of 1 mm are disposed at interval of 3 mm in the form of hound's-tooth check was employed.
- Example 5 The procedures of Example 5 were repeated except for performing the dust removing after the rubbing treatment using the device shown in FIG. 7 in the following manner, to prepare a continuous optical compensatory sheet.
- the transparent film was passed through between a back-up roller 72b (outer diameter: 50 mm) and a roller having an adsorptive layer of acrylic rubber 79b (outer diameter: 100 mm) which was disposed facing to the back-up roller, whereby dust on the reverse surface of the transparent film was removed.
- the continuous optical compensatory sheet was prepared for one hour.
- the resultant sheet was observed using a microscope (performed in the check step using device for check 13 (FIG. 1)). In more detail, it was observed whether point defect having a diameter of not less than 20 ⁇ m was present in the optical compensatory sheet of an area of 1 m 2 or not, and the number was accounted if the defect was present.
- the point defect is an area in which an image cannot be displayed.
- Two optical compensatory sheets (obtained from the continuous optical compensatory sheet mentioned above 1)) were attached to TN-type liquid crystal cell that the product of the difference between an extraordinary ray and an ordinary ray of the liquid crystal and the clearance between the substrates of the liquid crystal cell was 510 nm, and the twisted angle of the liquid crystal was 87 degrees, as shown in FIG. 15 (i.e., the optical compensatory sheets were attached in the same manner as RF1 and RF2). It were observed whether the displayed image had defect or not and whether the displayed image was uniform or not.
- optical compensatory sheet was prepared according to the continues steps of from a step of feeding a continuous transparent film to a step of winding up a resultant continuous optical compensatory sheet as shown in FIG. 1.
- a coating liquid for forming an orientation layer having the following composition was coated using a bar coater.
- the coating was conducted with moving the triacetyl cellulose film at a rate of 15 m/min., and then dried by passing the film through a drying zone (temperature: 60° C., length: 60 m) with moving the film at the same rate, to form a transparent resin layer having a thickness of 0.5 ⁇ m (film 4b in FIG. 1 was obtained).
- the surface of the resultant transparent resin layer was subjected to rubbing treatment with moving the triacetyl cellulose film at a speed of 15 m/min.
- the transparent film having the transparent resin layer 5b (FIG. 1) was moved at a speed of 15 m/min., and a surface of the transparent resin layer was rubbed by a rubbing roller (outer diameter: 150 mm; 8 of FIG. 1) rotating at 1,200 rpm in the reverse direction of the moving direction of the film and a tension for conveying the film of 4 kgf/cm (width of film), while the upper side of the film on the rubbing roller was depressed by a guide roller 6 (FIG. 1).
- a rubbing roller outer diameter: 150 mm; 8 of FIG. 1
- a coating liquid for forming layer of discotic compound was continuously coated on the orientation layer by the use of an wire-bar coating machine 10 (FIG. 1), with moving the triacetyl cellulose film having the orientation layer 4c (FIG. 1) at a speed of 15 m/min.
- the coating liquid for forming layer of discotic compound the same coating liquid as in Example 1 was employed.
- the above coating was conducted using as the wire-bar coating machine the machine shown in FIGS. 8 and 10 under the following conditions.
- Diameter of wire-bar 81 10 mm
- Viscosity 4.1 mPa.s
- the triacetyl cellulose film having the coated layer was passed through a drying zone 116 shown in FIG. 11 in which an air of a rate of 0.1 m/sec. was flowed in the same direction as that moving the film, at a rate of movement of 15 m/min. for 6 seconds, to dry the coated layer, and continuously the coated layer was passed through a heating zone (130° C.) 119 for orientation shown in FIG. 11 for 2 minutes to orient the discotic compound.
- the transparent film having the coated layer was passed through a UV zone 12 (FIG. 1) at a rate of movement of 15 m/min.
- the coated layer was exposed to UV light (a high-pressure mercury lamp (out-put power: 120 W/cm, emission length: 1.6 m)) in an intensity of illumination of 600 mW/cm 2 for one second, to cure the coated layer, and cooled to room temperature to form a cured layer of discotic layer.
- the film having the orientation layer and the layer of discotic compound was checked by measuring the optical characteristics of the film by the use of a device for check 13 (FIG. 1) with moving the film at a speed of 15 m/min. Then, a protective film 14 (FIG. 1) was superposed on the layer of discotic compound of the film using a laminator 15 (FIG. 1), and wound up by a winding machine. Thus, a continuous optical compensatory sheet in the form of roll, which comprises a transparent film, an orientation layer and a layer of discotic compound, was obtained.
- Example 8 The procedures of Example 8 were repeated except for changing the coating conditions of coating liquid for forming a layer of discotic compound (the cycling flow rate and residence time) in the following manner, to prepare a continuous optical compensatory sheet.
- Example 8 The procedures of Example 8 were repeated except for changing the coating conditions of coating liquid for forming a layer of discotic compound (the cycling flow rate and residence time) in the following manner, to prepare a continuous optical compensatory sheet.
- Streak on a coated surface produced when the coating liquid for forming a layer of discotic compound was coated was observed by eye.
- the coating was continuously performed for 100 minutes by repeating continuous coating of a continuous film of length of 300 m (i.e., such that the coating liquid is coated on a second film immediately after completion of coating of a first film). The streak produced during the coating operation was observed.
- optical compensatory sheets were attached to TN-type liquid crystal cell that the product of the difference between an extraordinary ray and an ordinary ray of the liquid crystal and the clearance between the substrates of the liquid crystal cell was 510 nm, and the twisted angle of the liquid crystal was 87 degrees, as shown in FIG. 15 (i.e., the optical compensatory sheets were attached in the same manner as RF1 and RF2).
- the optical compensatory sheets were prepared by employing an area having streak, if the streak was produced. It was observed the displayed image was uniform or not.
- optical compensatory sheet was prepared according to the continues steps of from a step of feeding a continuous transparent film to a step of winding up a resultant continuous optical compensatory sheet as shown in FIG. 1.
- a coating liquid for forming an orientation layer having the following composition was coated using an extrusion die.
- the coating was conducted with moving the triacetyl cellulose film at a rate of 15 m/min., and then dried by passing the film through a drying zone (temperature: 90° C., length: 60 m) with moving the film at the same rate, to form a transparent resin layer having a thickness of 0.5 ⁇ m (film 4b in FIG. 1 was obtained).
- a drying zone temperature: 90° C., length: 60 m
- the gap between the extrusion die 35 and the transparent film 34 was 200 ⁇ m, and the vacuum chamber 43 was kept at a pressure lower by 350 Pa than atmospheric pressure.
- a viscosity of the above coating liquid was 3.5 mpa.s (25° C.).
- the surface of the resultant transparent resin layer was subjected to rubbing treatment with moving the triacetyl cellulose film at a speed of 15 m/min.
- the transparent film having the transparent resin layer 5b (FIG. 1) was moved at a speed of 15 m/min., and a surface of the transparent resin layer was rubbed by a rubbing roller (outer diameter: 150 mm; 8 of FIG. 1) rotating at 1,200 rpm in the reverse direction of the moving direction of the film and a tension for conveying the film of 4 kgf/cm (width of film), while the upper side of the film on the rubbing roller was depressed by a guide roller 6 (FIG. 1).
- a rubbing roller outer diameter: 150 mm; 8 of FIG. 1
- a coating liquid for forming layer of discotic compound was continuously coated on the orientation layer by the use of an wire-bar coating machine 10 (FIG. 1), with moving the triacetyl cellulose film having the orientation layer 4c (FIG. 1) at a speed of 15 m/min.
- the coating liquid for forming layer of discotic compound the same coating liquid as in Example 1 was employed.
- the above coating liquid for forming a layer of discotic liquid (4 mpa.s) was coated using a wire-bar coater 111.
- the transparent film having the coated layer of discotic compound 114b was moved along a rectifiable plate 112 to a drying zone 116, and then moved to a heating zone 119 (distance (2 m) between the wire-bar coating machine 111 and the heating zone 119).
- a gas for drying was introduced into the drying zone 116 through a metallic netting 115a from an intake vent 113a (5mm ⁇ 450mm).
- the gas had a velocity of 0.15 m/sec. (25° C., 50%RH) in the direction of movement of the film at the metallic netting 115a.
- the gas introduced from an intake vent 113a was discharged at an exhaust vent 113b, and at the same time passed through the metallic netting 115a, a porous plate 118 and a metallic netting 115b to be discharged at a second exhaust vent 117.
- the provision of these porous plate 118 and a metallic netting 115b scarcely brings about marked variation of rate or direction of air.
- the transparent film having the coated layer of discotic compound 114b was moved between the wire-bar coating machine 111 and the heating zone 119 (total length: 2 m).
- the transparent film having the coated layer 114b after drying, was entered in the heating zone 119, and passed through the heating zone (130° C.) for 2 minutes to orient the discotic compound.
- the heating in the heating zone was conducted by blowing heated air (130° C.) at a velocity of 7 m/sec. on both sides of the transparent film having the coated layer, the air being introduced from air plenums 119a, 119b provided on both sides of the transparent film.
- air plenums 119a, 119b air plenums of air-plate type which are capable of blowing heated air and supporting the film, were employed.
- the transparent film having the oriented layer of discotic compound was passed through a UV zone 12 (FIG. 1) at a rate of movement of 15 m/min.
- the coated layer was exposed to UV light (a high-pressure mercury lamp (out-put power: 120 W/cm, emission length: 1.6 m)) in intensity of illumination of 600 mW/cm 2 for one second, to cure the oriented layer, and cooled to room temperature to form a cured layer of discotic compound having a thickness of 1.9 ⁇ m.
- the film having the orientation layer and the cured layer of discotic compound was checked by measuring the optical characteristics of the film by the use of a device for check 13 (FIG. 1) with moving the film at a speed of 15 m/min. Then, a protective film 14 (FIG. 1) was superposed on the layer of discotic compound of the film using a laminator 15 (FIG. 1), and wound up by a winding machine. Thus, a continuous optical compensatory sheet in the form of roll, which comprises a transparent film, an orientation layer and a cured layer of discotic compound, was obtained.
- Example 11 The procedures of Example 11 were repeated except for changing the velocity of the air at the metallic netting 115a in the drying zone from 0.15 m/sec. to 0.25 m/sec. to prepare a continuous optical compensatory sheet.
- Example 11 The procedures of Example 11 were repeated except for changing the velocity of the air at the metallic netting 115a in the drying zone from 0.15 m/sec. to 0.35 m/sec. to prepare a continuous optical compensatory sheet.
- Example 11 The procedures of Example 11 were repeated except for changing the velocity of the air at the metallic netting 115a in the drying zone from 0.15 m/sec. to 0.05 m/sec. to prepare a continuous optical compensatory sheet.
- Example 11 The procedures of Example 11 were repeated except for changing the velocity of the air at the metallic netting 115a in the drying zone from 0.15 m/sec. to 0.40 m/sec. to prepare a continuous optical compensatory sheet.
- Example 11 The procedures of Example 11 were repeated except for changing the velocity of the air at the metallic netting 115a in the drying zone from 0.15 m/sec. to 0.50 m/sec. to prepare a continuous optical compensatory
- the continuous optical compensatory sheet was observed using a polarizing microscope. In more detail, occurrence of schlieren or columnar phase of the optical compensatory sheet, which shows nonuniform orientation, was observed.
- optical compensatory sheets were attached to TN-type liquid crystal cell that the product of the difference between an extraordinary ray and an ordinary ray of the liquid crystal and the clearance between the substrates of the liquid crystal cell was 510 nm, and the twisted angle of the liquid crystal was 87 degrees, as shown in FIG. 15 (i.e., the optical compensatory sheets were attached in the same manner as RF1 and RF2).
- the optical compensatory sheets were prepared by employing an area having nonuniform orientation, if the nonuniform orientation was produced. It was observed the displayed image was uniform or not.
Abstract
Description
20≦{(nx+ny)/2-nz}×d≦400
T=V.sub.1 /Q
20≦{(nx+ny)/2-nz}×d≦400 (nm)
30≦{(nx +ny)/2-nz}×d≦150
|nx-ny|/|nx-nz|≦0.2
______________________________________ x y z (molar %) (molar %) (molar %) ______________________________________ Polymer No. A 87.8 0.2 12 Polymer No. B 87.997 0.003 12 Polymer No. C 87.86 0.14 12 Polymer No. D 87.94 0.06 12 Polymer No. E 86.9 1.1 12 Polymer No. F 98.5 0.5 1.0 Polymer No. G 97.8 0.2 2.0 Polymer No. H 96.5 2.5 1.0 Polymer No. I 94.9 4.1 1.0 ______________________________________ ##STR4## In the formula (1-2), n, x, y and z may be as follows:
______________________________________ n x(mol. %) y(mol. %) z(mol. %) ______________________________________ Polymer No. J 3 87.8 0.2 12 Polymer No.K 5 87.85 0.15 12 Polymer No. L 6 87.7 0.3 12 Polymer No. M 8 87.7 0.3 12 ______________________________________
50≦{(n.sub.3 +n.sub.2)/2-n.sub.1 }×D≦400(nm)
100≦{(n.sub.3 +n.sub.2)/2-n.sub.1 }×D≦400(nm)
______________________________________ Coating liquid for forming layer of discotic compound! 182 parts Discotic liquid crystalline compound (TE-8-(8, m = 4); compound previously mentioned) Ethylene glycol modified-trimethylol 18 parts propane triacrylate (V#360, available from Osaka Organic Chemical Industry Co., Ltd.) Acetylbutyrylcellulose 4 parts (CAB551-0.2, available from Eastman Chemical Co.) Photopolymerization initiator 6 part (Irgacure-907, available from Ciba-Geigy) Sensitizer 2 parts (Kayacure-DETX, available from Nippon Kayaku Co., Ltd.) Methyl ethyl ketone 343 parts ______________________________________
TABLE 1 ______________________________________ Evaluation of Yield Example Orientation image of LCD (%) ______________________________________ Ex. 1 Uniform orientation Uniform image 80 Ex. 2 Uniform orientation Uniform image 80 Ex. 3 Uniform orientation Uniform image 80 Ex. 4 Uniform orientation Uniform image 80 Co. Ex. 1 Locally nonuniform Observed a 40 orientation little nonuniform image ______________________________________
TABLE 2 ______________________________________ Defect of Uniformity Example Point Defect image of image ______________________________________ Ex. 5 None None Uniform Ex. 6 A little A little Slightly observed observed nonuniform Ex. 7 None None Uniform ______________________________________
______________________________________ Coating liquid for forming orientation layer! 10 parts Modified polyvinyl alcohol (previously mentioned polymer No. A) Water 371parts Methanol 119 parts Glutaraldehyde (crosslinking agent) 0.5 part ______________________________________
TABLE 3 ______________________________________ Occurrence Uniformity Example of streak of image ______________________________________ Ex. 8 None Uniform Ex. 9 Observed Slightly after 40 min. nonuniform Ex. 10 Observed Slightly after 80 min. nonuniform ______________________________________
______________________________________ Coating liquid for forming orientation layer! 10 parts Modified polyvinyl alcohol (previously mentioned polymer No. A) Water 371parts Methanol 119 parts Glutaraldehyde (crosslinking agent) 0.5 part ______________________________________
TABLE 4 ______________________________________ Velocity of air Velocity at metallic of air Uniformity Uniformity netting on the film of of Example (m/sec) (m/sec) orientation image ______________________________________ Ex. 11 0.15 -0.10 Uniform Uniform Ex. 12 0.25 0 Uniform Uniform Ex. 13 0.35 0.10 Uniform Uniforin Co. Ex. 2 0.05 -0.20 Slightly Slightly nonuniform nonuniform Co. Ex. 3 0.40 0.15 Slightly Slightly nonuniform nonuniform Co. Ex. 4 0.50 0.25 Greatly Greatly nonuniform nonuniform ______________________________________
Claims (8)
Applications Claiming Priority (8)
Application Number | Priority Date | Filing Date | Title |
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JP25024895A JPH0970568A (en) | 1995-09-04 | 1995-09-04 | Production of long-sized optical compensation sheet |
JP25024995A JP3616171B2 (en) | 1995-09-04 | 1995-09-04 | Manufacturing method of long optical compensation sheet |
JP7-250249 | 1995-09-04 | ||
JP7-250248 | 1995-09-04 | ||
JP7-255599 | 1995-09-06 | ||
JP7255599A JPH09166784A (en) | 1995-09-06 | 1995-09-06 | Production of long-sized optical compensation sheet |
JP25559895A JP3554619B2 (en) | 1995-09-06 | 1995-09-06 | Manufacturing method of long optical compensation sheet |
JP7-255598 | 1995-09-06 |
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US5853801A true US5853801A (en) | 1998-12-29 |
Family
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US08/697,888 Expired - Lifetime US5853801A (en) | 1995-09-04 | 1996-09-03 | Process for the preparation of continuous optical compensatory sheet |
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US (1) | US5853801A (en) |
KR (1) | KR100294521B1 (en) |
DE (2) | DE19655379B4 (en) |
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- 1996-09-03 US US08/697,888 patent/US5853801A/en not_active Expired - Lifetime
- 1996-09-04 KR KR1019960038218A patent/KR100294521B1/en not_active IP Right Cessation
- 1996-09-04 DE DE19655379A patent/DE19655379B4/en not_active Expired - Lifetime
- 1996-09-04 DE DE19635894A patent/DE19635894B4/en not_active Expired - Lifetime
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Also Published As
Publication number | Publication date |
---|---|
KR100294521B1 (en) | 2001-09-17 |
DE19655379B4 (en) | 2008-02-07 |
DE19635894B4 (en) | 2008-02-07 |
KR970016692A (en) | 1997-04-28 |
DE19635894A1 (en) | 1997-03-06 |
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